CN104388874A - Silver doped alumina ceramic coating and its making method - Google Patents

Silver doped alumina ceramic coating and its making method Download PDF

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Publication number
CN104388874A
CN104388874A CN201410541199.9A CN201410541199A CN104388874A CN 104388874 A CN104388874 A CN 104388874A CN 201410541199 A CN201410541199 A CN 201410541199A CN 104388874 A CN104388874 A CN 104388874A
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silver
powder
ceramic coating
alumina
preparation
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李恺
谢有桃
黄利平
郑学斌
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Shanghai Institute of Ceramics of CAS
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Shanghai Institute of Ceramics of CAS
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)
  • Materials For Medical Uses (AREA)

Abstract

The invention relates to a silver doped alumina ceramic coating and its making method. The alumina ceramic coating comprises alumina and silver, and the doping amount of silver is 1-5wt%.

Description

Alumina ceramic coating of a kind of Ag doping and preparation method thereof
Technical field
The present invention relates to a kind of wear-resisting Ag doping aluminum oxide coating layer good with anti-microbial property and preparation method thereof, be specifically related to a kind of using plasma spraying technology prepares Ag doping alumina ceramic coating at metal or alloy substrate surface.
Background technology
The aluminum oxide coating layer adopting plasma spraying method to prepare has good wear resistance, chemical stability and biocompatibility, obtains apply more widely in fields such as food machinery, chemical industry and medicine equipments.Aluminum oxide coating layer is applicable to food and the various mechanical part of chemical industry, is used as resistance to wearing and corrosion-resistant finishes.Aluminum oxide biological coating joint prosthesis can be used for the hip replacement of osteoporosis, fractured near end of thighbone or bone tumor patient.
But anti-microbial infection function of not having is one of main deficiency of aluminum oxide coating layer.The food origin disease great majority caused by microorganism are polluted by unwanted bacteria (as listeria spp and intestinal bacteria etc.) and cause due to food processing plant and foodstuff surface.If the material surface anti-microbial property with Food Contact can be given, pathogenic micro-organism so effectively can be suppressed to adhere to and growth, avoid the further propagation of food origin disease.Along with a large amount of joint prosthesis implant into body, its implant infections relating caused has become one of sixty-four dollar question in 21 century medical field.Implant infections relating not only extends wound healing time, also can cause limbs disability and dysfunction time serious.For reducing implant infections relating odds, be necessary to develop the biological coating with antibacterial.
Summary of the invention
The present invention is intended to overcome the defect of existing ceramic coating at antibiosis, the invention provides alumina ceramic coating of a kind of Ag doping and preparation method thereof.
The invention provides a kind of alumina ceramic coating of Ag doping, the composition of described alumina ceramic coating comprises aluminum oxide and silver, and wherein, the doping of silver is 1-5wt%.
Preferably, the thickness of described coating is 10 microns ~ 400 microns.
Again, present invention also offers a kind of preparation method of above-mentioned alumina ceramic coating, described method comprises:
1) employing silver powder, alumina powder jointed preparation meet silver/aluminum oxide mixed powder that is silver-colored in described alumina-ceramic, alumina ration relation;
2) using plasma spraying technology, by step 1) silver/aluminum oxide mixed powder of preparing, spray on base material, obtain the alumina ceramic coating of described Ag doping.
Preferably, step 1) in, adopt planetary ball mill mixing silver powder, alumina powder jointed.
Preferably, step 1) in, silver powder and alumina powder jointed total mass, be 1:(1-3 with the mass ratio of zirconium oxide abrasive ball); The rotating speed of ball milling is 300 ~ 500r/ minute, and Ball-milling Time is 60 ~ 300 minutes; After ball milling is complete, powder sieves and dries at 100 ~ 120 DEG C.
Preferably, step 2) in, described base material before spraying through pre-treatment, wherein, pre-treatment is: after first substrate surface being carried out sandblasting (preferably under 0.2 ~ 0.5MPa pressure) or sand papering, then by base material in ethanol solution ultrasonic 1 ~ 2 time, each 3 ~ 5 minutes, then by base material 100 ~ 120 DEG C of dryings 1 ~ 2 hour.
Preferably, step 2) in, the processing parameter of plasma spray technology is: plasma gas Ar flow is 35 ~ 50slpm; Plasma gas H 2flow is 8 ~ 18slpm; Powder carrier gas Ar flow is 1.5 ~ 5slpm; Spray distance is 100 ~ 330mm; Spray power is 30 ~ 55kW; Spray time is 10 ~ 40 minutes; Powder feeding rate is 8.0 ~ 30gmin -1; Described slpm refers to standard liter/min.
Preferably, step 2) in, described base material is metal or alloy base material.
Beneficial effect of the present invention:
Ceramic coating of the present invention has obvious antibacterial effect to intestinal bacteria, and sterilization rate reaches more than 99%; Frictional wear experiment proves, the wear resistance of carrying silver-colored alumina ceramic coating is obviously better than pure phase aluminum oxide coating layer, and silver-colored adds the frictional coefficient and average wear rate that reduce ceramic coating.
Accompanying drawing explanation
Fig. 1 shows the XRD figure spectrum of powder and the corresponding ceramic coating prepared in an embodiment of the invention, wherein, a is the XRD figure spectrum of the powder prepared in one embodiment of the present invention, and b is the XRD figure spectrum of the ceramic coating prepared in one embodiment of the present invention;
Fig. 2 show prepare in an embodiment of the invention carry silver-colored alumina ceramic coating, Ti-6Al-4V coating and pure alumina ceramic coating to colibacillary antibacterial effect figure, wherein, a is the visible colonies figure that intestinal bacteria and Ti-6Al-4V act on after 24 hours; B is intestinal bacteria and the visible colonies figure of alumina ceramic coating effect after 24 hours; C is intestinal bacteria and year visible colonies figure of silver-colored alumina ceramic coating effect after 24 hours;
Fig. 3 a shows the growing state effect diagram of Ti-6Al-4V to mouse bone-forming cell system MC3T3-E1;
Fig. 3 b shows the growing state effect diagram of aluminum oxide coating layer to mouse bone-forming cell system MC3T3-E1;
Fig. 3 c show prepare in an embodiment of the invention carry silver-colored aluminum oxide coating layer to the growing state effect diagram of mouse bone-forming cell system MC3T3-E1;
Fig. 4 shows ceramic coating and the alumina ceramic coating of the prior art stable state frictional coefficient comparison diagram respectively under three kinds of load 20N, 30N, 40N prepared in one embodiment of the present invention;
Fig. 5 shows the ceramic coating and the average wear rate comparison diagram of alumina ceramic coating of the prior art under three kinds of load 20N, 30N, 40N prepared in one embodiment of the present invention;
Fig. 6 shows and carries silver-colored aluminum oxide coating layer (Ag doping amount is 6wt%) the growing state effect diagram to mouse bone-forming cell system MC3T3-E1.
Embodiment
Further illustrate the present invention below in conjunction with accompanying drawing and following embodiment, should be understood that accompanying drawing and following embodiment are only for illustration of the present invention, and unrestricted the present invention.
The invention discloses a kind of wear-resisting ceramic coating good with anti-microbial property and preparation method thereof, wherein, described coating formation, in the surface of the base material of metal or alloy material, is the alumina ceramic coating of Ag doping, and in described coating, the massfraction of silver is 1 ~ 5%.Coating of the present invention not only has excellent germ resistance, and has the wear resistance being obviously better than pure phase aluminum oxide coating layer, can be widely used in the fields such as food machinery, chemical industry and medicine equipment.
Silver-colored massfraction is that the silver/aluminum oxide mixed powder of 1 ~ 5% is sprayed on pretreated metal or alloy substrate surface by using plasma spraying coating process.
Described silver-colored massfraction is the silver/aluminum oxide mixed powder of 1 ~ 5%, powder is obtained by mechanical attrition method: by silver powder, alumina powder jointedly to mix with zirconium oxide abrasive ball, put into the grinding pot of tetrafluoroethylene, ball milling is carried out in planetary ball mill, sieve and dry the powder obtaining spraying, wherein the mass ratio of mixed powder and zirconium oxide abrasive ball is 1:1 ~ 1:3.The rotating speed of ball milling is 300 ~ 500r/min, and Ball-milling Time is 60 ~ 300 minutes, then crosses 80 mesh sieves and dries at 100 ~ 120 DEG C.
Prepared by using plasma spraying technology, spraying parameter is: plasma gas Ar flow is 35 ~ 50slpm; Plasma gas H 2flow is 8 ~ 18slpm; Powder carrier gas Ar flow is 1.5 ~ 5slpm; Spray distance is 100 ~ 330mm; Spray power is 30 ~ 55kW; Powder feeding rate is 8.0 ~ 30gmin -1; Described slpm refers to standard liter/min.
Described metal or alloy substrate surface pre-treatment, refers to by substrate surface after pressure is sandblasting under 0.2 ~ 0.5MPa or sand papering, in ethanol solution ultrasonic 1 ~ 2 time, each 3 ~ 5 minutes, then 100 ~ 120 DEG C of dryings 1 ~ 2 hour.
Silver is conventional inorganic antiseptic, has the advantages such as efficient and broad-spectrum antimicrobial, is widely used in multiple fields such as medicine equipment, hospital, water purification system, food product pack, food fresh-keeping, sanitary facility.Recent studies have found that, in Calucium Silicate powder biological coating, add a small amount of silver, can give coating good antimicrobial property, the Ag doping Calucium Silicate powder base coating being 3% as silver-colored massfraction all reaches 99% to streptococcus aureus and colibacillary sterilization rate.
Ceramic coating of the present invention has obvious antibacterial effect to intestinal bacteria, and sterilization rate reaches more than 99%; Frictional wear experiment proves, the wear resistance of carrying silver-colored alumina ceramic coating is obviously better than pure phase aluminum oxide coating layer, and silver-colored adds the frictional coefficient and average wear rate that reduce ceramic coating.
The germ resistance that the present invention is raising ceramic coating and wear resistance provide a kind of effective solution; Further, method of the present invention have simple to operate, efficiency is high, favorable repeatability, be applicable to the advantage such as large-scale production.
Exemplify embodiment below further to describe the present invention in detail.Should understand equally; following examples are only used to further illustrate the present invention; can not be interpreted as limiting the scope of the invention, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention.The processing parameter etc. that following example is concrete is also only an example in OK range, and namely those skilled in the art can be done in suitable scope by explanation herein and select, and do not really want the concrete numerical value being defined in Examples below.
Embodiment 1
A, mechanical attrition method prepare powder
Silver powder, alumina powder jointed and zirconium oxide abrasive ball are mixed according to the mass ratio of 5:95:200, put into the grinding pot of tetrafluoroethylene, ball milling is carried out in planetary ball mill, rotational speed of ball-mill is 400r/min, Ball-milling Time is 300min, cross 80 mesh sieves afterwards, at 110 DEG C, dry to obtain mixed powder, for subsequent use.
B, plasma spray process prepare ceramic coating
After Ti-6Al-4V alloy surface being carried out sandblasting (pressure 0.3MPa), ultrasonic cleaning 2 times in ethanol solution, each 4 minutes, then 110 DEG C of dryings 1 hour, for subsequent use;
Using plasma spraying coating process, mixed powder is sprayed to the titanium alloy surface after process and obtain the ceramic coating that thickness is 160 microns, wherein, plasma spray process parameter is as follows: plasma gas Ar flow is 40slpm, plasma gas H 2flow is 10slpm, and mixed powder carrier gas Ar flow is 3.5slpm, and spray distance is 100mm, and spray power is 42kW, and spray time is 21 minutes, and powder feeding rate is 24gmin -1.
The XRD figure spectrum of silver as shown in Figure 1/aluminum oxide mixed powder and corresponding ceramic coating is visible, and the composition structure of coating and powder considerable change does not occur.
C, coating anti-microbial property are tested
Adopt the anti-microbial property of colony counting method detection by quantitative material: select intestinal bacteria as test bacterial classification.Get strain inoculation in nutrient agar medium surface, cultivate 24 hours in thermostat container.With reference to bacterium standard opacity tube, intestinal bacteria being diluted to concentration is 2 × 10 6the bacterium liquid of individual bacterium/ml.Through Ti-6Al-4V, aluminum oxide coating layer, year each dropping in the silver-colored alumina ceramic coating surface 50 μ l bacterium liquid of the 30mm × 10mm × 2mm of high-temperature sterilization, stick the preservative film through alcohol disinfecting, 37 DEG C are incubated 24 hours.Dropped into respectively by sample in the test tube that 5ml PBS is housed, eddy current shakes 30 seconds, gets 0.5ml liquid in test tube successively, carries out 10 -1with 10 -2dilution, then, respectively gets 0.2ml and is inoculated in nutrient agar medium, cultivate 48 hours.In Fig. 2, c carries silver-colored alumina ceramic coating to colibacillary antibacterial effect figure, and compared with control piece, carry silver-colored alumina ceramic coating and have obvious antibacterial effect, antibiotic rate reaches more than 99%.
D, coating Cytotoxic evaluation
Sample vat liquor is adopted to evaluate the cytotoxicity of coating.By Ti-6Al-4V, aluminum oxide coating layer, carry silver-colored alumina ceramic coating with 2cm 2the ratio of/ml (surface area of sample/amount of solution) is soaked in α-MEM substratum, 37 DEG C, 5%CO 2cultivate 24 hours under environment, collect vat liquor, degerming with 0.22 μm of filtering with microporous membrane, standby cell experiment is used.The mouse bone-forming cell system MC3T3-E1 adding a small amount of α-MEM substratum is made 1 × 10 4individual cell/ml suspension.Cultivate 24 hours in 96 hole polyethylene culture plates, remove nutrient solution, add Ti-6Al-4V, aluminum oxide coating layer respectively, carry silver-colored alumina ceramic coating vat liquor 50 μ l.37 DEG C, 5%CO 2cultivate 24 hours under environment.Inverted phase contrast microscope is utilized to observe the growing state of MC3T3-E1 cell;
Find out from Fig. 3 a, in Ti-6Al-4V vat liquor, cell is fusoid viable cell shape characteristic, and Growth of Cells is vigorous, aluminum oxide coating layer (Fig. 3 b) and carry cell in silver-colored aluminum oxide coating layer (Fig. 3 c) vat liquor and present similar pattern.The above results tentatively shows, and carries silver-colored aluminum oxide coating layer to MC3T3-E1 cell without overt toxicity.
The frictional wear experiment of ceramic coating under E, different loads effect
Surperficial fine grinding is carried out to year silver-colored aluminum oxide coating layer and alumina ceramic coating sample and (adopts Al 2o 3fine grinding cream, particle diameter 10 μm, speed υ=1m/s, pressure F=40 ~ 60N, time t=0.5 hour) and surface finish process (diamond is milled cream, particle diameter 1 μm, speed υ=1.5m/s, pressure F=40 ~ 60N, time t=1 ~ 2 hour), make ceramic coating surface roughness (Ra) be down to less than 0.5 μm.Subsequently, year silver-colored alumina ceramic coating after polishing and alumina ceramic coating are arranged on UMT-3 friction wear testing machine respectively (purchased from CETR, the U.S.) on, select ball dish pattern, it is as follows that friction parameter is set: vertical load is respectively 2Kg (i.e. F=20N), 3Kg (i.e. F=30N) and 4Kg (i.e. F=40N), to abrading-ball departure distance 15mm (radius r of namely sliding), disk rotational speed 130r/min (w=130), wearing-in period 50 minutes (t=50 minute).The relation of record the friction coefficient distance, calculates stable state frictional coefficient.After test terminates, use T-8000C roughness tester (Wave, Germany) (the polishing scratch sectional area of each ceramic coating sample test 10 different positionss calculates the average wear rate (10 of ceramic coating according to formula (I) for the wear area of test polishing scratch -6mm 3/ Nm, i.e. unit distance unit load lower volume loss).
νs = s ave · 1 F · L = s ave · 2 πr F · 2 πrwt = s ave F · wt - - - ( I )
Wherein, S averepresent average abrasion area, l represents polishing scratch girth, L representative wearing and tearing distance.
Stable state frictional coefficient result as shown in Figure 4, under load 20N, 30N and 40N effect, alumina ceramic coating stable state frictional coefficient is respectively 0.421 ± 0.013,0.311 ± 0.011,0.348 ± 0.011, and silver/alumina composite ceramic coating stable state frictional coefficient is respectively 0.387 ± 0.004,0.284 ± 0.012,0.299 ± 0.001.By more known, under 20N, 30N and 40N tri-kinds of different loads, the stable state frictional coefficient of silver/alumina composite coating is all less than pure phase aluminum oxide coating layer.As shown in Figure 5, under load 20N, 30N and 40N effect, the average wear rate of silver/alumina composite coating is all lower than pure phase aluminum oxide coating layer for average wear rate result.
Comparative example 1
Adopt preparation condition in embodiment 1 (difference is only that the mass ratio of silver powder and aluminum oxide powder is 6:94), prepare the alumina ceramic coating that Ag doping amount is 6wt%;
In comparative example 1, the Ag doping amount of preparation is the alumina ceramic coating of 6wt%, carries out coating Cytotoxic evaluation same in embodiment 1.Carry in silver-colored aluminum oxide coating layer vat liquor and cultivate the MC3T3-E1 cell morphology of 24 hours as shown in Figure 6, a large amount of apoptosis.This may be because in coating, silver content is higher, result in cytotoxicity.

Claims (8)

1. an alumina ceramic coating for Ag doping, is characterized in that, the composition of described alumina ceramic coating comprises aluminum oxide and silver, and wherein, the doping of silver is 1-5wt%.
2. ceramic coating according to claim 1, is characterized in that, the thickness of described coating is 10 microns ~ 400 microns.
3. a preparation method for alumina ceramic coating described in claim 1 or 2, is characterized in that, described method comprises:
1) employing silver powder, alumina powder jointed preparation meet silver/aluminum oxide mixed powder that is silver-colored in described alumina-ceramic, alumina ration relation;
2) using plasma spraying technology, silver step 1) prepared/aluminum oxide mixed powder, sprays on base material, obtains the alumina ceramic coating of described Ag doping.
4. preparation method according to claim 3, is characterized in that, in step 1), adopts planetary ball mill mixing silver powder, alumina powder jointed.
5. preparation method according to claim 4, is characterized in that, in step 1), silver powder and alumina powder jointed total mass, is 1:(1-3 with the mass ratio of zirconium oxide abrasive ball); The rotating speed of ball milling is 300-500 r/ minute, and Ball-milling Time is 60-300 minute; After ball milling is complete, powder sieves and dries at 100-120 DEG C.
6. according to described preparation method arbitrary in claim 3-5, it is characterized in that, step 2) in, described base material before spraying through pre-treatment, wherein, pre-treatment is: after first substrate surface being carried out sandblasting or sand papering, then by base material in ethanol solution ultrasonic 1-2 time, each 3-5 minute, then by base material at 100-120 DEG C of dry 1-2 hour.
7., according to described preparation method arbitrary in claim 3-6, it is characterized in that, step 2) in, the processing parameter of plasma spray technology is: plasma gas Ar flow is 35 ~ 50 slpm; Plasma gas H 2flow is 8 ~ 18 slpm; Powder carrier gas Ar flow is 1.5 ~ 5 slpm; Spray distance is 100 ~ 330 mm; Spray power is 30 ~ 55 kW; Spray time is 10 ~ 40 minutes; Powder feeding rate is 8.0 ~ 30 gmin -1; Described slpm refers to standard liter/min.
8., according to described preparation method arbitrary in claim 3-7, it is characterized in that, step 2) in, described base material is metal or alloy base material.
CN201410541199.9A 2014-10-14 2014-10-14 Silver doped alumina ceramic coating and its making method Pending CN104388874A (en)

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Cited By (6)

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CN105239356A (en) * 2015-09-05 2016-01-13 苏州宏久航空防热材料科技有限公司 Composite ceramic coating for surface of SiC fiber and preparation method thereof
CN106668942A (en) * 2015-11-05 2017-05-17 中国科学院上海硅酸盐研究所 Production method of boron-doped calcium silicate bioactive coating
CN109183110A (en) * 2018-11-27 2019-01-11 中国科学院海洋研究所 A kind of micro-arc oxidation preparation antifouling Integrative Coating of aluminium alloy surface anti-corrosion and preparation method thereof
CN110205576A (en) * 2019-04-25 2019-09-06 中国科学院兰州化学物理研究所 A kind of preparation method of vacuum low abrasion 8YSZ+Ag ceramet coating
CN111921007A (en) * 2020-07-23 2020-11-13 北京大学第三医院（北京大学第三临床医学院） Surface modified zirconia material with long-acting antibacterial effect and preparation method and application thereof
CN114150267A (en) * 2021-11-26 2022-03-08 西安交通大学 Preparation method of alumina/silver nanoparticle layer/alumina multilayer antibacterial film

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105239356A (en) * 2015-09-05 2016-01-13 苏州宏久航空防热材料科技有限公司 Composite ceramic coating for surface of SiC fiber and preparation method thereof
CN106668942A (en) * 2015-11-05 2017-05-17 中国科学院上海硅酸盐研究所 Production method of boron-doped calcium silicate bioactive coating
CN109183110A (en) * 2018-11-27 2019-01-11 中国科学院海洋研究所 A kind of micro-arc oxidation preparation antifouling Integrative Coating of aluminium alloy surface anti-corrosion and preparation method thereof
CN110205576A (en) * 2019-04-25 2019-09-06 中国科学院兰州化学物理研究所 A kind of preparation method of vacuum low abrasion 8YSZ+Ag ceramet coating
CN111921007A (en) * 2020-07-23 2020-11-13 北京大学第三医院（北京大学第三临床医学院） Surface modified zirconia material with long-acting antibacterial effect and preparation method and application thereof
CN114150267A (en) * 2021-11-26 2022-03-08 西安交通大学 Preparation method of alumina/silver nanoparticle layer/alumina multilayer antibacterial film
CN114150267B (en) * 2021-11-26 2022-08-16 西安交通大学 Preparation method of alumina/silver nanoparticle layer/alumina multilayer antibacterial film

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